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Measurement 46 (2013) 161170

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Measurement
journal homepage: www.elsevier.com/locate/measurement

The measurement of thermal conductivity variation with temperature


for solid materials
S. Aksz a, E. ztrk b, N. Marasl c,
a
Nevsehir University, Faculty of Arts and Sciences, Department of Physics, 50300 Nevsehir, Turkey
b
Kocaeli University, Faculty of Arts and Sciences, Department of Physics, 41380 Kocaeli, Turkey
c
Erciyes University, Faculty of Sciences, Department of Physics, 38039 Kayseri, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: An apparatus was designed to routinely measure the thermal conductivity variation with
Received 22 April 2012 temperature for solid materials. The apparatus was calibrated by measuring the thermal
Received in revised form 1 June 2012 conductivity variations with temperature for aluminum, zinc, tin and indium metals. The
Accepted 5 June 2012
variations of thermal conductivity with temperature for the Zn-[x] wt.% Sb alloys (x = 10,
Available online 26 June 2012
20, 30 and 40) were then measured by using the linear heat ow apparatus designed in
present work. From experimental results it can be concluded that the linear heat ow
Keywords:
apparatus can be used to measure thermal conductivity variation with temperature for
A. Metals
D. Thermal conductivity
multi component metallic alloys as well as pure metallic materials and for any kind of
D. Electrical conductivity alloys. Variations of electrical conductivity with temperature for the Zn-[x] wt.% Sb alloys
were determined from the WiedemannFranz (WF) equation by using the measured val-
ues of thermal conductivity. Dependencies of the thermal and electrical conductivities on
composition of Sb in the ZnSb alloys were also investigated. According to present exper-
imental results, the thermal conductivity and electrical conductivity for the Zn-[x] wt.% Sb
alloys decrease with increasing the temperature and the composition of Sb.
2012 Elsevier Ltd. All rights reserved.

1. Introduction by measuring the rate of heat ow per unit area and the
temperature gradient. In non-steady state methods of
In the experimental determination of the thermal con- measurement, the temperature distribution in the speci-
ductivity of solids, a number of different methods of mea- men varies with time, and the measurement of the rate
surement are required for different ranges of temperature of temperature change, which normally determines the
and for various classes of materials having different ranges thermal diffusivity, replaces the measurement of the rate
of thermal conductivity values. A particular method may of heat ow. The thermal conductivity is then calculated
thus be preferable over-others for a given material and from the thermal diffusivity with a further knowledge of
temperature range. the density and specic heat of the materials [1].
The various methods for the measurement of thermal Many attempts have been made to determine the ther-
conductivity fall into two categories: steady state and mal conductivity values of solid and liquid phases in vari-
non-steady state methods. In steady state methods of mea- ous materials by using different methods. One of the
surement, the specimen is subjected to a temperature pro- common techniques for measuring the thermal conductiv-
le that is time invariant; after equilibrium has been ity of solids is the longitudinal heat ow method. In the
reached; the thermal conductivity is determined directly longitudinal heat ow methods, the experimental arrange-
ment is so designed that the ow of heat is only in the axial
Corresponding author. Tel.: +90 352 437 49 01x33114; fax: +90 352
direction of a road specimen. Under steady-state condition
437 49 33. and assuming no radial heat loss or gain, thermal conduc-
E-mail address: marasli@erciyes.edu.tr (N. Marasl). tivity is determined by the following expression from

0263-2241/$ - see front matter 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.measurement.2012.06.003
162 S. Aksz et al. / Measurement 46 (2013) 161170

one-dimensional FourierBiot heat conduction equation 2. Experimental procedure


[1,2]:
2.1. Experimental apparatus
Q DT
K 1
A DX As mentioned above, a linear heat ow apparatus was
designed to routinely measure the thermal conductivity
where K is the thermal conductivity of solid, Q is the rate of variation with temperature for solid materials. The linear
heat ow or input power ows through to specimen, A is heat ow apparatus consists of hot stage, cold stage and
the cross-sectional area of the specimen, DX = X2  X1 is sample holder as shown in Fig. 1.
the distance between points of temperature measurements The hot-stage is comprised of two brass plates which are
for T1 and T2 and DT = T2  T1 is the temperature difference resistively heated by NiCr wires, insulated in alumina tubes
between X2 and X1 points. and integrally threaded through the plates of the hot stage.
There are several different types of apparatus, all A total of 1000 mm of heater wire, 0.5 mm in diameter was
employing the longitudinal heat ow methods. The longi- used in the hot-stage, providing a maximum power of
tudinal heat ow methods are a steady state methods 4500 W at 220 V AC. To maximize the thermal stability of
and the classication is mainly based upon: absolute or the hot-stage, a transformer was placed in the supply cir-
comparative methods. Rod method is one of the most com- cuit, stepping the maximum current down to 4 A. A fully
mon absolute methods and suitable for good conductors. proportional thermistor-based control system was imple-
The specimen is in the form of a relatively rod so as to pro- mented, employing a control thermocouple within the
duce an appreciable temperature drop along the specimen hot-stage. The temperature of the hot-stage was controlled
for precise measurement. In this method, a source of heat to an accuracy of 0.01 K with a Eurotherm 2604 type con-
at a constant temperature is supplied at the one end of troller. The hot stage can be operated up to 773 K degrees.
the rod and ows axially through the rod to other end, The cold-stage design is similar to that of the hot-stage.
where a heat sink at a lower constant temperature is lo- However, cooling is achieved by using a Poly Science digi-
cated. Radial heat loss or gain of rod should be negligible. tal 9102 model heating/refrigerating circulating bath con-
In order to determine the thermal conductivity from Eq. taining an aqueous ethylene glycol solution. The
(1), it is necessary to measure the rate of heat ow into temperature of the circulating baths was kept constant at
and/or out of the rod, cross-sectional area, the tempera- 278 K with an accuracy of 0.01 K.
tures of at least two points along the rod and the distance To get linear temperature gradient into specimen, the
between points of temperature measurements. For mea- distance between the hot stage and cold stage was kept
surements at lower (cryogenic) temperatures, radial heat typically 10 mm. Hot and cold stages were placed with a
loss does not constitute a serious problem, and thermal space of 10 mm on an insulating plate and the insulating
insulation and guard heaters are normally not necessary plate was then vertically xed as the hot stage is at top
[35]. For measurements at higher temperatures, radial of the insulating plate and the cold stage is at bottom to
heat loss becomes serious problem because radiant heat prevent convection effect on heat conduction into speci-
transfer increases rapidly with temperature. This method, men and get a constant linear temperature gradient into
as used for measurements at higher temperatures has been specimen as shown in Fig. 1.
reviewed and discussed by Laubitz [6] and Flynn [7]. Mea- Sample holder consists of two copper plates as shown in
surements of thermal conductivity at higher temperatures Fig. 2. Two holes in 10 mm depth and 8 mm diameter were
have been made for different kind of materials [815]. drilled at cross sections of cold and hot copper plates to
Recently, we have embarked on research pertaining to place the specimen between the hot and cold stages and
the measurement of thermal conductivity variation with get good heat conduction trough to specimen. At the same
temperature of metals and multi-components of metallic time, a hole in 3 mm diameter through bottom cold copper
alloys. So attention is given to the thermal conductivity plate was also drilled to insert the measurements thermo-
and electrical conductivity at high temperature required couples into specimen. The ends of specimen were tightly
as input data in heat transfer and solidication simulators. tted into holes at the cold and hot copper plates. Thermo-
The aim of present work was to modify the rod method to couples were then placed into specimen by inserting ther-
measure thermal conductivity variation with temperature. mocouples through hole at the cold plate as shown in
For this purpose, a linear heat ow apparatus was designed Fig. 1. Then, top and bottom copper plates include the
and calibrated by measuring the thermal conductivity var- specimen were placed together into hot and cold stages.
iation with temperature for the aluminum, zinc, tin and in-
dium metals. Then, the thermal conductivity variations
with temperature for the Zn-[x] wt.% Sb alloys (x = 10, 20, 2.2. Specimen preparation and processing
30 and 40) were measured with the linear heat ow appa-
ratus designed in present work. The variations of electrical A thin-walled graphite crucible, 12.0 mm OD  8.0 mm
conductivity with temperature for same alloys were also ID  50 mm in length was made by drilling out a graphite
determined from the WiedemannFranz (WF) equation rod of 12 mm in diameter and 250 mm in length. A hole,
by using the measured values of thermal conductivity. 1.2 mm in diameter was drilled at the bottom of crucible
Dependencies of the thermal and electrical conductivities for thermocouples alumina tube as shown in Fig. 3.
on composition of Sb in the ZnSb alloys were also ZnSb binary system shows an eutectic phase equilibria
investigated. in the range of compositions 057 wt.% Sb. The eutectic
S. Aksz et al. / Measurement 46 (2013) 161170 163

Insulating plate Multimeter


-----AC V
Power input

Hot stage Controller thermocouple

Cold stage

-----AC I
Heating/ Multimeter
refrigerating
circulator

Fluid inlet
Fluid outlet

Measurement thermocouples

Data logger
Transformer
Temperature controller
Computer

Fig. 1. Block diagram of linear heat ow apparatus.

60 mm

Hot copper plate


12 mm

45 mm
8 mm 10 mm 8 mm
Cold copper plate
10 mm

3 mm
Measurement thermocouples 3 mm
4 mm

10 mm

Positions of measurement thermocouples into specimen

Fig. 2. Schematic illustration of copper plates and thermocouples positions into specimen.

melting temperature of ZnSb system is about 684 K. Be- furnace by using metals of purity of 99.99%. After stirring,
low the eutectic temperature, the ZnSb binary system the molten alloy was poured into a graphite crucible, held
consists of solid Zn and solid e (Sb-43 wt.% Zn). Thus, com- in a specially constructed casting furnace at approximately
position of ZnSb alloys were chosen to be 10, 20, 30 and 50 K above the melting point of the metals. The molten
40 wt.% Sb to see the affect of alloying Sb element on the metals were then directionally solidied from bottom to
thermal conductivity of ZnSb alloy. top to ensure that the crucible was completely lled.
Tin, zinc, indium, aluminum and Zn-[x] wt.% Sb alloys The solidied specimen was removed from the graphite
(x = 10, 20, 30 and 40) were separately melted in a vacuum crucible and cut into lengths typically 30 mm. The 30 mm
164 S. Aksz et al. / Measurement 46 (2013) 161170

12 mm was measured with optical microscope to determine the


8 mm cross-sectional area (pr2). The temperatures of stationary
thermocouples were recorded with a Pico TC-08 data-log-
ger during the heat and the difference of temperature be-
tween two thermocouples, DT was read from the data
Graphite crucible
logger records. The distance between the two thermocou-
17 mm ples was measured from the photograph of the thermocou-
ples positions. In this experimental technique, the main
Specimen
difculty was the measurement of heat ow rate into rod
specimen. To overcame this difculty, the input powers gi-
ven to experimental system (heater) for without specimen
(QWOS) and with specimen (QWS) were separately deter-
Alumina tube mined by measuring the voltage drops at the end of heater
and currents passing through the heater under the steady
23 mm state conditions. Heat ow rate into rod specimen (Q) for
each steady state condition was assumed to be the differ-
ence between the values of QWS and QWOS in present work.
After all desired temperature measurements had been
completed during the heat, the cooling procedure was
started in same steps down to room temperature.
10 mm The sample was then removed from the linear heat ow
apparatus and the longitudinal section of the specimen
was examined for porosity, cracks, and casting defects to
Fig. 3. Schematic illustration of specimen. make sure that these would not introduce any errors to
the measurements.
length of specimen was placed into the linear heat ow Variations of thermal conductivity with temperature for
apparatus. Both ends of specimen (10 mm length) were in- the Al, Zn, Sn, In and Zn-[x] wt.% Sb alloys (x = 10, 20, 30
serted into holes at the hot and cold stages. Thus, a space of and 40) were determined from Eq. (1) by using the mea-
10 mm between the hot stage and cold stage was adjusted sured values of A, Q = QWS  QWOS, DT and DX.
to get a linear temperature gradient into specimen and
prevent radial heat loss of rod. The temperatures at differ- 2.3. Experimental error analysis in the thermal conductivity
ent parts of the specimen were measured with mineral measurement
insulated metal sheathed, 0.25 mm in diameter K type
(nickel chromiumnickel aluminum) three thermocouples, The estimated experimental error in the measurement
xed within the specimen with a spacing of 23 mm as of K is the sum of the fractional uncertainty of the mea-
shown in Fig. 2. Three thermocouples were placed with a surements of heat ow rate, temperature difference, cross
spacing of 23 mm and stuck together with silicone elasto- sectional area of specimen and thermocouple positions
mer glue. Before inserting the thermocouples into speci- which can be expressed as
men, the photograph of thermocouples positions was
taken to measure the distance between the thermocouples DK s DQ DT  DA DX

K Q DT A X 2
(DX) with optical microscope. All thermocouples were s
then inserted together into alumina tubes, 1.2 mm
OD  1.0 mm ID  20 mm in length and the ends of the
2.3.1. Fractional uncertainty in the heat ow rate
thermocouples were then connected to the measurement
measurement
unit which is consisted of data-logger and computer.
As mentioned above, the heat ow rate into specimen
The specimen was heated from one side by using a hot
was assumed to be the difference between the values of
stage in steps of 40 K up to 10 K below the melting temper-
QWS and QWOS for each steady state condition, i.e.
atures of the materials and the other side of specimen was
Q = QWS  QWOS. Typical data for measurements of heat
kept cool by using a cold stage to get linear temperature
ow rates are given in Table 1. Thus, the estimated exper-
gradient. As mentioned above the temperature of hot stage
imental error in the measurement of Q is the sum of the
was controlled to an accuracy of 0.01 K with a Eurotherm
fractional uncertainty in the measurements of QWS and
2604 type controller and the temperature of cold stage was
QWOS and can be expressed as
kept constant to an accuracy of 0.01 K with a Poly Science

digital 9102 model heating/refrigerating circulating bath. DQ DQ WS DQ WOS
3
The specimen was kept at steady state condition for at Q Q Q
WS WOS
least 2 h for each temperature.
In order to determine the thermal conductivity from The input power is expressed as
Eq. (1), it is necessary to measure the rate of heat ow into
Q V I 4
the rod, cross-sectional area, the temperatures of at least
two points along the rod and the distance between points where V and I are the potential drop at the end of hot
of temperature measurements. The radius of rod specimen stage (heater) and the current passing through the heater,
S. Aksz et al. / Measurement 46 (2013) 161170 165

Table 1
Typical experimental data to determine heat ow rate into aluminum rod specimen at different temperatures.

Temperature (K) IWOS (A) VWOS (V) QWOS (W) IWS (A) VWS (V) QWS (W) Q = QWS  QWOS (W)
313 0.77 7.59 5.87 0.9 9.1 8.3 2.4
353 1.39 13.04 18.12 1.8 17.6 31.2 13.1
393 1.95 19.34 37.71 2.3 23.6 54.9 17.2
433 2.35 23.50 55.23 2.9 28.5 82.1 26.9
473 2.88 29.62 85.32 3.2 35.0 112.6 27.3
513 3.28 33.35 109.46 3.7 37.9 140.2 30.8
553 3.56 36.79 130.91 4.1 41.8 169.7 38.8
593 3.87 39.75 153.66 4.4 45.8 202.7 49.1
633 4.28 44.05 188.46 4.8 49.6 237.1 48.7
673 4.66 47.86 222.77 5.2 53.9 277.7 54.9

IWOS: Current passing through to heater without specimen; IWS: Current passing through to heater with specimen; VWOS: Potential drop at the ends of heater
without specimen; VWS: Potential drop at the ends of heater with specimen; QWOS: Input power given to heater without specimen; QWS: Input power given
to heater with specimen; Q: Heat ow rate through to specimen.

respectively under the steady state condition. The fractional ple readings (DT) at the same points of the specimen must
uncertainty in the power measurement can be expressed as be known or measured to determine the uncertainty of

DQ DV DI temperature measurement. To determine the difference
5
Q V I of the thermocouple readings, the thermocouples were cal-
ibrated by detecting the melting point of a metallic mate-
Potential drop and the current were measured with a rial. The difference between the two thermocouple
HewlettPackard 34401-A multimeter. The variations in readings (DT) were in the range of 0.030.2 K at different
the current reading (DI) were 0.02 A at different temper- temperatures [16]. As can be seen from Table 2, the tem-
atures. Typical data to determine heat ow rates through perature differences into the specimens (DT = T1  T2)
to aluminum rod at different temperatures are given in were in the range of 1.230.6 K at different temperatures.
Table 1. As can be seen from Table 1, the currents passing The uncertainties in the temperature measurement into
through to specimen were in the range of 0.95.2 A at dif- the specimen are in the range of 0.62.5% at different tem-
ferent temperatures. The uncertainties in the current mea- peratures. The estimated error in the temperature mea-
surements are in the range of 0.32.2%. The estimated error surement into the specimen is about 2.5%.
in the current measurement is about 4.4%.
The variations in the potential drop readings (DV) were 2.3.3. The fractional uncertainty in the measurement of cross-
0.03 V at different temperatures. As can be seen from Ta- sectional area (A) and the xed distances (X1, X2)
ble 1, the potential drops at the end of hot stage were in The cross sectional area of specimen (A) is pr2 and the
the range of 9.153.9 V. The uncertainties in the potential fractional uncertainty in the cross sectional surface mea-
drop measurements are in the range of 0.050.3% at differ- surement is expressed as
ent temperatures. The estimated error in the potential drop
DA
measurement is about 0.6%. 2 Dr 6
Thus, the total fractional uncertainty in heat ow rate
A r
measurement is about 5%.
where r is the radius of specimen. The radius of specimen is
measured to be 4000 lm by using an optical microscope
2.3.2. Fractional uncertainty in the measurement of with an accuracy of 10 lm. Thus, the uncertainty in the
temperature difference between two thermocouples, DT=T1 measurement of radius or cross sectional area of specimen
 T2 at the setting temperature is less than 0.5%.
The temperature of the specimen was measured with K The distance between two thermocouple positions
type thermocouples. The difference of the two thermocou- (DX = X2  X1) was also measured by using an optical

Table 2
Experimental data in the measurements of thermal conductivity variations with temperature for the aluminum, zinc, indium and tin.

Temperature (K) Aluminum (Al) Zinc (Zn) Indium (In) Tin (Sn)
K (W/Km) DT (K) Q (W) K (W/Km) DT (K) Q (W) K (W/Km) DT (K) Q (W) K (W/Km) DT (K) Q (W)
313 238.0 1.2 2.4 117.6 1.7 1.2 82.7 2.4 3.3 66.9 4.7 5.3
353 234.3 6.7 13.1 113.3 2.8 2.1 82.0 4.8 6.6 65.0 8.9 9.7
393 232.0 8.9 17.2 111.7 5.1 5.6 80.8 6.1 8.3 63.0 13.6 14.4
433 230.5 13.9 26.9 110.3 8.5 8.3 80.0 8.4 11.2 61.2 19.4 19.8
473 228.0 14.3 27.3 105.6 9.9 10.1 80.0 10.0 13.4 59.4 24.9 24.8
513 224.1 16.4 30.8 104.0 24.6 32.5 78.9 12.6 16.6
553 221.2 20.9 38.80 100.8 33.5 47.1
593 218.6 26.8 49.06 99.5 40.4 56.1
633 216.7 26.8 48.67 97.6 45.6 60.2
673 214.3 30.6 54.92

K: Thermal conductivity of specimen (W/Km); DT: Temperature difference into specimen (K); Q: Heat ow rate into specimen (W).
166 S. Aksz et al. / Measurement 46 (2013) 161170

microscope with an accuracy of 10 lm. The measured va- semiconductors. Electrical conductivity is a measure of a
lue of DX = X2  X1 is about 3000 lm. The fractional uncer- materials ability to conduct an electric current and is
tainty in the measurement of the xed distance is about one of the primary physical properties of materials such
0.3%. as thermal conductivity, specic heat and thermal expan-
Therefore the total fractional uncertainty in the mea- sion. The relationship between the thermal conductivity
surements of thermal conductivity in present work is and the electrical conductivity of metals is established by
about 9%. the WiedemannFranz equation [19], which is based on
the fact that heat and electrical transport both involve
2.4. Determination of the thermal temperature coefcient the free electrons in the metal as:
Ke
For a given composition, the dependence of the thermal LT 9
r
conductivity of the solid phase on temperature is linear
and the thermal temperature coefcient, aTTC is expressed where L is the constant of proportionality, which is called
as [17,18] the Lorenz number. The value of L is 2.45  108 WX/K2.
The variation of electrical conductivity (r) with tempera-
K  K0 1 DK ture can be determined from the WiedemannFranz equa-
aTTC 7
K 0 T  T 0 K 0 DT tion by using the measured values of K.
where K is the thermal conductivity at the temperature of
T, K0 is the thermal conductivity at the room temperature, 2.6. Determination of electrical temperature coefcient
T0 = 300 K and aTTC is the thermal temperature coefcient.
This means that the thermal temperature coefcient, aTTC The electrical conductivity is strongly dependent on
can be obtained from the graph of thermal conductivity temperature. In metals, electrical conductivity decreases
variations with temperature and also given in Table 3. with increasing temperature, whereas in semiconductors,
electrical conductivity increases with increasing tempera-
2.5. Determination of electrical conductivity ture. The dependence of electrical conductivity on temper-
ature is often expressed as a slope in the electrical
Heat in solid is conducted by various carriers: electrons, conductivity versus temperature graph and can be given
lattice waves or phonons, magnetic excitations, and, in as:
some cases, electromagnetic radiation. The total thermal r  r0 1 Dr
conductivity is additively composed of contributions from aETC 10
r0 T  T 0 r0 DT
each type of carrier. The principal carriers of heat in metals
are electron and lattice waves, leading to an overall ther- where r is the electrical conductivity at the temperature
mal conductivity (T), r0 is the electrical conductivity at the room tempera-
ture, T0 = 300 K and aETC is the electrical temperature
K Ke Kg 8 coefcient.
where Ke is the electronic component and Kg is the lattice
component. 3. Results and discussions
Generally Kg of metals, alloys and semimetals is of mag-
nitude comparable to the lattice thermal conductivity of 3.1. Calibration of linear heat ow apparatus
insulators of corresponding elastic properties, except at
low temperature where phononelectron interaction re- As mentioned above, the rod method is one of the most
duces Kg in metals. The relative importance of Ke and Kg common absolute method and suitable for good conduc-
thus depends on the magnitude of Kg. The electronic com- tors. In this method, a source of heat at a constant temper-
ponent often parallels the electrical conductivity and the ature is supplied at the one end of the rod and ows axially
electrical conductivity is highest in pure metals, reduced through the rod to other end, where a heat sink at a lower
in the case of alloys and, even lower in semimetals and constant temperature is located. Radial heat loss or gain of

Table 3
Some thermal and electrical properties of tin, zinc, indium, aluminum, and Zn-[x] wt.% Sb alloys (x = 10, 20, 30 and 40) at their melting temperature.

Metals Melting Thermal conductivity Thermal temperature Electrical Electrical


temperature (K) K (W/Km) coefcient conductivity temperature
aTTC (K1) r  108 (1/Xm) coefcient aETC (K1)
Tin (Sn) 505 57.80 0.000692 0.0413 0.002554
Zinc (Zn) 692 93.07 0.000524 0.0406 0.001874
Indium (In) 429 78.27 0.000444 0.0718 0.002710
Aluminum (Al) 933 237.35 0.000273 0.0115 0.001518
Zn-10 wt.% Sb 682 55.68 0.000477 0.0181 0.002073
Zn-20 wt.% Sb 682 42.93 0.000433 0.0139 0.002068
Zn-30 wt.% Sb 682 30.86 0.000767 0.0080 0.002238
Zn-40 wt.% Sb 682 21.68 0.000881 0.0049 0.002308
S. Aksz et al. / Measurement 46 (2013) 161170 167

rod should be negligible. In order to determine the thermal In addition, the thermal temperature coefcient of the Zn,
conductivity with rod method, it is necessary to measure Sn, In and Al were also found to be 0.000524, 0.000692,
the rate of heat ow into and/or out of the rod, cross sec- 0.0004444 and 0.000273 K1, respectively from Fig. 4.
tional area, the temperatures of at least two points along A comparison of the variation of thermal conductivity, K
the rod and the distance between points of temperature with temperature for the Zn, Sn, In and Al measured in
measurements. Main difculty in the rod method was the present work with the variation of thermal conductivity,
measurement of heat ow rate into and/or out of the rod. K with temperature for same metals measured in previous
In present work, this problem was overcome by measuring work [17] is given in Fig. 4. As can be seen from Fig. 4, the
the input powers given to experimental system (heater) for lines of thermal conductivity variation with temperature
with specimen (QWS) and without specimen (QWOS) at each measured in present work are slightly above than the lines
steady state conditions. of thermal conductivity variations with temperature for
For condence of experimental technique, the calibra- the same metals measured in previous works [17] and re-
tion of experimental apparatus must be made. For this pur- sults are in a good agreement with the previous works in
pose, Al, Zn, Sn, and In metals were chosen as test materials the range of experimental error. This means that the pres-
because of their thermal conductivity variations with tem- ent experimental technique is capable to easily and sensi-
perature are well known [17]. Same sized specimens for tively determine the variation of thermal conductivity with
Zn, Sn, In and Al were heated from one side by using a temperature for solid materials.
hot stage in steps of 40 K up to 10 K below the melting
temperature of the metals. The other side of specimens 3.2. Dependency of the thermal conductivity on the
was kept cool by using a cold stage to get linear tempera- temperature and composition of Sb in the Zn-[x] wt.% Sb alloys
ture gradient during the annealing period. The specimen
was kept at steady state condition for at least 2 h for each The eutectic melting temperature of Zn-[x] wt.% Sb bin-
temperature. The temperature difference between two ary system is about 684 K [20]. Zn-[x] wt.% Sb eutectic sys-
thermocouples (DT) for each temperature (steady state tem consists of solid e (Sb3Zn4) and solid Zn according to
condition) was read from the data logger record. The ther- the composition of Sb up to 57 wt.% Sb below the eutectic
mal conductivity of specimens for each steady state condi- melting temperature [20]. In present work, the variations
tion were obtained from Eq. (1) by using the measured of thermal conductivity with temperature for the Zn-
values of A, Q, DT and DX. [x] wt.% Sb alloys (x = 10, 20, 30 and 40) were also mea-
The variations of thermal conductivity with tempera- sured with the linear heat ow apparatus designed in pres-
ture for the Zn, Sn, In and Al were given in Table 2 and plot- ent work. Experimental results are given in Table 4 and
ted in Fig. 4. The thermal conductivity of Zn, Sn, In and Al at plotted in Fig. 5.
their melting temperature were found to be 93.07, 57.80, A comparison of the values of K for the Zn-[x] wt.% Sb al-
78.27 and 237.35 W/km, respectively by extrapolation the loys measured in present work with the values of K for Sb
thermal conductivity curves to the melting temperatures. [17] and Sn [17] are also given in Fig. 5. As can be seen from
Thermal Conductivity (W/Km)
Thermal Conductivity (W/Km)

250 70
Al [17] 68 Sn [17]
Al [PW] Sn [PW]
240 66
64
230 62
60
220 58
56
210 54
200 300 400 500 600 700 280 320 360 400 440 480 520
Temperature (K) Temperature (K)
Thermal Conductivity (W/Km)

Thermal Conductivity (W/Km)

84
115
In [17] Zn [17]
82 In [PW]
110 Zn [PW]

80
105
78
100
76
95
74
300 320 340 360 380 400 420 300 350 400 450 500 550 600 650
Temperature (K) Temperature (K)

Fig. 4. Variations of thermal conductivity with temperature for the Al, Sn, In and Zn metals.
168 S. Aksz et al. / Measurement 46 (2013) 161170

Table 4
Thermal conductivity variations with temperature for Zn-[x] wt.% Sb alloys (x = 10, 20, 30 and 40).

Temperature (K) Zn-10 wt.% Sb Zn-20 wt.% Sb Zn-30 wt.% Sb Zn-40 wt.% Sb
K (W/Km) DT (K) Q (W) K (W/Km) DT (K) Q (W) K (W/Km) DT (K) Q (W) K (W/Km) DT (K) Q (W)
313 67.19 3.04 3.43 50.93 4.38 3.74 43.07 3.27 2.36 31.92 5.22 2.79
353 66.15 7.27 8.06 50.69 8.94 7.59 41.77 7.10 4.96 30.82 12.90 6.66
393 65.61 11.11 12.21 49.54 13.41 11.12 40.34 11.39 7.69 29.94 16.86 8.46
433 64.43 14.70 15.86 48.78 16.43 13.42 39.78 14.50 9.66 28.97 23.18 11.25
473 63.17 23.13 24.46 48.05 19.17 15.42 38.20 18.08 11.56 27.13 29.98 13.62
513 60.47 23.86 24.16 47.79 22.87 18.31 37.91 21.02 13.34 26.52 36.93 16.40
553 59.57 28.08 28.01 45.11 26.88 20.31 33.81 27.30 15.46 25.56 44.10 18.88

K: Thermal conductivity of specimen (W/Km); DT: Temperature difference into specimen (K); Q: Heat ow rate into specimen (W).

Fig. 5, the value of K decreases with increasing the temper-


70
ature. The measured lines of thermal conductivity varia-
313
tions with temperature for the Zn-[x] wt.% Sb alloys lie

Thermal Conductivity (W/Km)


353
between the lines of thermal conductivity variation with 393
60 433
temperature for Sb [17] and Zn [17]. As mentioned above, 473
513
the Zn-[x] wt.% Sb eutectic system consists co-exit two dif- 553
50
ferent solid phases as solid e (Sb3Zn4) and solid Zn below
the eutectic melting temperature. If the composition of Sb
in the ZnSb increases the mole fraction of intermetallic 40
phase (Sb3Zn4) increases. Thus, the lines of thermal conduc-
tivity variation with temperature for that alloys should be
below the line of thermal conductivity variation with tem- 30
perature for zinc. The values of K for the Zn-[x] wt.% Sb al-
loys (x = 10, 20, 30 and 40) at their melting temperature 20
were obtained to be 55.68, 42.93, 30.86, and 21.68 W/km, 5 10 15 20 25 30 35 40 45
respectively by extrapolating the thermal conductivity Composition (wt.%Sb)
curves to their melting temperature as shown in Fig. 5. In
Fig. 6. The variations of thermal conductivity with composition of Sb in
addition, the thermal temperature coefcient of the Zn-
the Zn-[x] wt.% Sb alloys at different temperatures.
[x] wt.% Sb alloys (x = 10, 20, 30 and 40) were also found
to be, 0.000477, 0.000433, 0.000767 and 0.000881 K1,
respectively from Fig. 5. 3.3. Dependency of the electrical conductivity on the
The thermal conductivity variations with composition of temperature and composition of Sb
Sb in the Zn-[x] wt.% Sb alloys (x = 10, 20, 30 and 40) were
plotted in Fig. 6 at different temperatures (313, 353, 393, The experimental error in the measurements of thermal
433, 473, 513 and 553 K). As can be seen from Fig. 6, the conductivity variation with temperature is about 9% by
thermal conductivity of Zn-[x] wt.% Sb alloys exponentially using the radial heat ow apparatus. Experimental error
decrease with increasing the composition of Sb. in the measurement of electrical conductivity is generally
higher than 9%. Thus, the variations of electrical conductiv-
ity with temperature determined from the Wiedemann
Franz (WF) equation for the Zn-[x] wt.% Sb alloys are plot-
ted in Fig. 7. There is no information about on the electrical
120
Thermal Conductivity (W/Km)

conductivity variations with temperature for the Zn-


Sb
100 Zn [x] wt.% Sb alloys. Thus, a comparison of the variations of
Zn-10 wt.%Sb
Zn-20 wt.%Sb
electrical conductivity with temperature determined from
80 Zn-30 wt.%Sb the WF equation for the Zn-[x] wt.% Sb alloys with the
Zn-40 wt.%Sb variations of electrical conductivity with temperature for
60 Sb and Zn measured in previous work [21] is also given
in Fig. 7. As can be seen from Fig. 7, the value of r for
40 the Zn-[x] wt.% Sb alloys decreases with increasing the
temperature and the calculated lines of r from the WF
20 equation for the Zn-[x] wt.% Sb alloys lie between the lines
of electrical conductivity variations with temperature for
0 Sb [21] and Zn [21].
200 300 400 500 600 700
The values of r for the Zn-[x] wt.% Sb alloys (x = 10, 20, 30
Temperature (K)
and 40) at their melting temperatures were obtained to be
Fig. 5. Variations of thermal conductivity with temperature for the Zn 18.1  103, 13.9  103, 8  103, and 4.9  103 (Xm)1,
[17], Sb [17] and Zn-[x] wt.% Sb alloys. respectively by extrapolating the electrical conductivity
S. Aksz et al. / Measurement 46 (2013) 161170 169

alloys change, as in pure materials, not only with temper-


ature but also it changes by compositions of alloys.
The measurement of thermal conductivity variation
with temperature for solid is difcult and very expensive.
To overcome these problems a linear heat ow apparatus
was designed to routinely measure the thermal conductiv-
ity variation with temperature for solids. To get a linear
temperature gradient into specimen, one side of specimens
was heated by using a hot stage and the other side of spec-
imens was kept cool by using a cold stage. The main dif-
culty in the experimental technique was the measurement
of heat ow rate into the rod specimen. This problem was
overcome by measuring the input powers given to experi-
mental system (heater) for with specimen (QWS) and with-
out specimen (QWOS) at each steady state conditions.
Fig. 7. Variations of electrical conductivity with temperature for the Zn
The variations of thermal conductivity with tempera-
[21], Sb [21] and Zn-[x] wt.% Sb alloys. ture were measured for the Zn, Sn, In and Al by using the
linear heat ow apparatus and the results were compared
with the known values of thermal conductivity variation
with temperature for the same metals measured in previ-
ous work [17]. From the comparison of present experimen-
tal results with previous results, it can be concluded that
the results are in a good agreement with the previous
works in the range of experimental error. The present
experimental technique has the advantages of simpler
apparatus, easier specimen fabrication and easier opera-
tion and can be used to determine the thermal conductiv-
ity variation with temperature for metals as well as
metallic and organic alloys. Present experimental tech-
nique might also be used to determine the thermal con-
ductivity variation with temperature for liquid materials.
Dependency of thermal conductivity of the Zn-[x] wt.%
Sb alloys on the temperature and composition of Sb were
investigated by using a linear heat ow apparatus designed
in present work. The thermal conductivities of the Zn-
Fig. 8. The variations of electrical conductivity with composition of Sb in
the Zn-[x] wt.% Sb alloys at different temperatures. [x] wt.% Sb alloys decrease with increasing the tempera-
ture and composition of Sb.
curves to their melting temperature. The electrical tempera- The electrical conductivity variations with temperature
ture coefcients for the Zn-[x] wt.% Sb alloys (x = 10, 20, 30 for the Zn-[x] wt.% Sb alloys were determined from the
and 40) were found to be 0.002073, 0.002068, 0.002238 WiedemannFranz (WF) equation by using the measured
and 0.002308 K1, respectively from Fig. 7 and also given values of thermal conductivity for same alloys. The electri-
in Table 4. cal conductivities of Zn-[x] wt.% Sb alloys decrease with
The variations of electrical conductivity with composi- increasing the temperature and composition of Sb.
tions of Sb in the Zn-[x] wt.% Sb alloys determined from
the WF equation were plotted in Fig. 8 at different tem-
peratures (313, 353, 393, 433, 473, 513 and 553 K). As Acknowledgements
can be seen from Fig. 8, the electrical conductivity of Zn-
[x] wt.% Sb alloys linearly decreases with increasing the This project was supported by the Erciyes University
composition of Sb. Scientic Research Project Unit under Contract No.: FBA-
10-3297 and the Nevsehir University Scientic Research
Project Unit under Contract No.: 2010/15. Authors would
like to thank to the Erciyes University Scientic Research
4. Conclusions
Project Unit and Nevsehir University Scientic Research
Project Unit for their nancial support.
The thermal conductivity (K) and electrical conductivity
(r) are the main fundamental properties of materials such
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